Liquid chromatography determination of citalopram enantiomers using beta-cyclodextrin as a chiral mobile phase additive

A reliable and specific method for the determination of citalopram enantiomers was developed and validated. Chromatographic resolution of citalopram enantiomers was made on a Shim-pack (5 microm particle size) cyanopropyl column with beta-cyclodextrin (beta-CD) as an effective chiral mobile phase additive. The composition of the mobile phase was (90 + 10, v/v) aqueous 0.1% triethylammonium acetate buffer, pH 4.0 (adjusted with acetic acid), and acetonitrile, containing 12 mM beta-CD. The flow rate was 0.8 mL/min with ultraviolet detection at 240 nm. The effects of the mobile phase composition, concentration of beta-CD, and pH of the triethylammonium acetate buffer on peak shape and resolution of the enantiomers were investigated. The calibration graphs were linear (r = 0.9999, n = 8) in the range of 1-40 microg/mL for S(+) citalopram and R-(-) citalopram. The limit of detection values were 5.51 x 10(-3) and 4.35 x 10(-3) pg/mL, while the limit of quantification values were found to be 1.84 x 10(-2) and 1.45 x 10(-2) microg/mL for S-(+) citalopram and R-(-) citalopram, respectively.     

ChemInform Abstract: Barium Dierbium(III) Tetrasulfide.

Orange needles of BaEr₂S₄ are obtained during an investigation of the Ba/Er/U/S system by solid state reaction of a mixture of ²³⁸U, Er, BaS, and S in the ratio 1:1:3:3 (evacuated C‐coated fused silica tube, 1273 K, 8 d, cooling rate 3 K/h) together with black crystals of Sb₂S₃ and US₂.     

A microstructure-based model for time-dependent mechanics of multi-layered soft tissues and its application to intervertebral disc annulus

Meccanica - In recent experimental studies an unusual time-dependent transversal behavior of the annulus fibrosus of the intervertebral disc mainly caused by the coupling between mechanics and...     

Efficient algorithms for physical layer security in one-way relay systems

Wireless Networks - In this paper, we solve two problems aiming at improving the secure communications in a one-way relay system. The system under consideration consists of one source, one...     

Calibration of hot-wire probes using non-uniform mean velocity profiles

A simple iterative procedure is illustrated here to overcome two problems frequently encountered in hot-wire anemometry: (1) the calibration of hot wires at low velocity and (2) to account for the wall-proximity correction in the actual measurements. The low-velocity calibration method used an iterative correction procedure based on laminar pipe velocity profiles. It is shown that the use of this approach, together with a simple wall proximity correction procedure, provides a simple and accurate calibration of both single and cross hot wires, and gives reliable measurements.     

Kinetic properties of aryldialkylphosphatase immobilised on chitosan myristic acid nanogel

Organophosphorus (OP) compounds are extensively used in agricultural practice for pest management. However, their residues have a long half-life in the ecosystem as well as in the agro-products, posing a serious threat to human and animal health. Aryldialkylphosphatase (EC 3.1.8.1) is widely used in detoxification procedures. In the present study, aryldialkylphosphatase was immobilised on synthesised cross-linked nano-sized gel particles, also known as nanogels, in order to enhance the enzyme’s physicochemical properties. Accordingly, a new nanogel consisting of chitosan and myristic acid (CMA nanogel) was synthesised and characterised by way of Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The aryldialkylphosphatase-CMA nanogel conjugate was then assayed by FTIR, and its physicochemical characteristics were also investigated. The data obtained from SEM and TEM showed the nanogels to be homogenous spherical particles less than 50 nm in diameter. The proper formation of the nanogel and nanobioconjugate was also confirmed by FTIR spectra. In comparison with the free enzyme, the pH and thermal stability of the aryldialkylphosphatase were enhanced by the covalent immobilisation. Moreover, the immobilised enzyme could maintain approximately half of its activity over more than one month. The kinetic parameters of the aryldialkylphosphatase-CMA nanogel conjugate were also shown to undergo remarkable improvements, hence the synthesised CMA-nanogel could act as a promising support for aryldialkylphosphatase immobilisation. It is suggested that the aryldialkylphosphatase-CMA nanogel could be used for detoxifying paraoxon; a nerve agent. Further clinical experiments are underway.     

One‐Pot Domino Synthesis of 3‐Amino‐1,2‐dihydroisoquinolines

A one‐pot method for the synthesis of 3‐amino‐7‐nitro‐1,2‐dihydroisoquinoline‐4‐carbonitriles from 2‐chloro‐5‐nitrobenzylamines and malononitrile has been developed.     

Latrunculin with a highly oxidized thiazolidinone ring: structure assignment and actin docking

A new latrunculin, oxalatrunculin B (3), was isolated from Red Sea sponge Negombata corticata. Extensive spectroscopic analysis revealed an unprecedented heterocycle in which the rare thiazolidinone ring found in latrunculins was oxidized with three additional oxygens. An actin polymerization inhibition assay agreed with MM-PBSA free energy calculations that 3 binds more weakly than latrunculin B to actin. Significant antifungal and anticancer activity of 3 was found, suggesting an alternate target in addition to actin for latrunculin bioactivity.     

Design,synthesis and anticoagulant activity of new flexible calix[8]arene sulfonic acids

Four new calix[8]arene sulfonic acids (2a-b, 3a-b) were synthesized. The anticoagulant activity and POM virtual screening of these flexible calixarenes have been established.